Apparatus for recovery of solid material from continuous contact filtration process



OGL 2l .1952 J. E. PENlcK ETAL 2,614,

APPARATUS FOR RECOVERY OF SOLID MATERIAL FROM CONTINUOUS CONTACT FILTR SFiled June 22. 1949 ATION PROCES 2 SHEETS-SHEET L SGHW S5. umsl Sm hOct. 21,. 1952 E; PENlcK ErAL APPARATUS FOR RECOVERY OF SOLID MATERIALFROM CONTINUOUS CONTACT FILTRATION PROCESS` Filed June 22, 1949zsHEETs-SHEET 2 4Patented Oct. 21, 1952 2,614,653 l APPARATUSFORARECOVERY OF SOLID MA- TERIAL FROM CONTINUOUS CONTACT vFIL'rRA'rIoNPROCESS Joe E. Penick, Woodbury, and Eric V. Bergstrom,

Short Hills, N. J., assignorsto Socony-Vacuum, l Oil Company,Incorporated, a. corporationv ofy N etv York Application June 22, 1949,serial No. 100,588 f 1 claim.' (C1.` 18s-.34)

This application -is directed vto an limproved process for ,thecontinuous contacting of adsorbent vpowdered Imaterial with oilsv andrefersmore .particularly v:totl'le continuous revivication `of spentpowdered'adsorbent material which has :beenused for treating liquidoils. An example ofthe type of lprocess to which the invention:appertains isvthe .contact refining of lubricating .oils ,to removelgum-,forming compounds, color bodies and other objectionable material.

The materialgenerally usedas the pulverized Aor powderedadsorbentdisclays such as fullers earth, Silica gels. bauxites,bentonite, montmorillonites, activated charcoal, and certain synthetic.associations of silica andalumina to which other .materials such Vascertain metallic oxides may be added. This material should be pulverizedto a 'grai11;siz e `which will pass through a 100 mesh vTyler screen andpreferably within the rangeof about 15G-400 mesh size. l I In thesecontact filtration processes, the lpowdered material becomes fouled bythe deposition ofcarbonaceous material and oily constituents .uponitssurface. By the-use-of solvents such as naphtha, low boiling .alcoholsand ketones, some of the contaminants can be removed,but the op-.eration is-too costly and inefficient to be considered commerciallypractical. The usual custom y `inthis artis tolsubject the spentadsorbent material to al combination of steaming and naphtha-mashingtoeffect removal of the .oily constituents ,from the adsorbent,after which-thenaphtha may be distilled off in a rotary drumkilnfollowedfby burning of the contaminants in anothermechanically drivenkiln. This .procedure hasnot proved satisfactory because `of `the `highheat cost involved in distilling the naphtha fromthe adsorbent particlesand because the eliciencyof the adsorbent for treating oils was to agreat ,extent lojst in the burning regeneration. The latter difficultyis in a', largepart due tolthe impossibility of providing ,adequatetemperature control of the adsorbent by burning' regeneration j inIrotary drum ykilns and similarjkilnsemployed commercially. QA. majorobject ,ofthis -invention is. to .continuouslyiregenerate finecontactmaterial with Va a minimum loss of entrained .materalinvthe exitgases. This yand other objectsolfthis invention will be made apparent bythe following description read inview of the attached drawings, in which`Figure 1 yshows a scherriaticview, highly diagrammatic, of apparatusadapted to continuously revivifylspent adsorbent material, fouled fromuse inacontact filtration process ;l and Figure z is a diagrammaticsketch, showing' the relationship of the elementsof a continuous contact`I lltrationH process,`the elements being reprevsentedin block .form

In Athe contact ltration of oils for decoloriza tion, etc., such as,thedecolorization of petroleum oils, forexample, vpulverized contactmaterial is admittedto a chamber containing the o il'. The mixture isagitated to assure even distribution. The adSQrbent particles-Rick 11pthe b'ictior'lable material from the O iLand the filtered oil'canberemoved continuouslyl from they chamber. .When thev particles ofadsorbent-become fouled to the `extentthat their filtering. efficiencyis reduced materially, they 'are removed from .the chamber. Thefouledcontact materialfis' passed through one or more solvent Washings,and ltering steps,

and is then admitted to apparatus shown on Figure 1 described herebelowrReferring nowtoligure 1, contact material .from the naphtha'lter ispassed through conduit Il)l to the pressure seal conveyer Il.- Theconveyer, of 'themRedler'type,.permits the maintenance of a pressuredifferential between its en- 25 vtrance and exitfandl is readilyadaptable to this invention, although other suitable conveyers areavailable. f f i,

The contact material is fed-throughconduit I2 vfrom theconveyer 'IlWinto lthe vdryer 13. The dryer I3 lmay suitably'be a l,verticallymounted vessel of circular cross-section. 'Steam is admitvted to thelower section .of dryer I3, through con- Vduit I4 to maintainthecontactmaterialwithin Athe dryer in ebullient motion. The steam may be admittedto the dryer i3 through a multiplicity of conduits I4,.suit'ably spacedacross'fthe bottom Qof the vessel toprovide more-evendistribution asinstalled in the conduits i4 Itoi increase ythe velocity o f thejsteamvto provide'bette'r mixing in thedryen The steam has *a dual purpose inthat inaddition .to jproyidingsupport forth'e contact material, 'it actsasse' kstripping fiuidremoving.

vsome of the more volatile materials from the .contact material;A"Ofcourselthe, steam admitted to the dryer I3.' .through conduitsvIlmaybesufliciently hot to 'impart `,atleast some offtheheatto thecontact jmaterial to volatlize someiof the Yheavier oily constituents onthe surface thereof.

In addition, a heating vcoil l5 'is'located near the Ybottom of the'dryer" l`3"to 'provide vlieatwhen de,- sirfid.' steam is admitted'treu'shthe'coil rl sity means' of `the 'steamjconduitl 6,1,tlie amount'being controlled ybyvalvgeijll heat-in the orrori 'heating coils I8located in the lower `section of the dryer. The source of heat for thecoils I8 Will be described in detail hereinafter. The coils I8 may becoiled tubes ora bank of conduits adapted to provide suitable heattransfer. vThe steam and vapors within the dryer may be removed rom anoutlet near the top thereof, and conducted through a conduit I9 to thequench condenser 20. n

The quench condenser 2i! is a vertically mounted vessel, which may be ofcircular crosssection. The condenser 26 contains heat eX- changer tubesand may be supplied with coolant uid through conduit 2|. The coolant isremoved through the conduit 22. changer may be of conventional verticaltube design with top and bottom headers, and consequently is notdescribed in detail, The coolant may suitably be water. moved from thedryer I8, admitted to the top of the quench condenser 20, passvdownwardly through the condenser 23 VHand' are cooled by contactwiththe exchanger tubes. The cooled vapors pass into a separator 23 locatedbelow the quench condenser, and communicating therewith. The vapors,`converted to liquids by Vthe cooling action of the condenser, settle inother material rises tothe top and is removed throughy conduit 2S.HThenaphtha may be rec`ycled"'through conduit 21 controlled by valve 28to the top of the quench condenser to permit better separation.'Thenaphtha is sprayed into the top of the l"condenser 2B throughnozzles, distributed across' the vessel, to aid in the condensation andseparation of the vapors removed from. the dryer I3.v The naphtha isthereafter removed to the naphtha iilter for reuse through-conduit 3B,controlled by valve 24. The heavier liquids and'solids which pass to thebottom of the separator 23 are Withdrawn through conduit 3I and returnedto the naphtha lter for further treatment.

The dried contact material is removed from the bottom of the dryerthrough the conduits 32, 32. are installed in the outlet conduits 32, 32to prevent packing or bridging 'of the contact material therein.A Thekflow of material in conduits 32, 32 may be controlled by valves 34, 34,but is normally controlled by continuous feeders 35, 35 of the starvalve type. The contact material is thereafter vfed intoconduit 36 fortransmission to the regenerator, 31. The contact material in conduit 36is carried'by a suitable lift gas, which may be steam or aninert gasadmitted through conduit 33 controlled by valve 39. The lift gas mayalso be air admitted" to the conduit by the blower 4B, controlled by thevalve 4 I .f

The regenerator '31 is fa, vertically mounted vessel of circular,rectangular or other suitable cross-section. The contact materialsupported byj the lift gas is admitted to the bottom of the regeneratorthrough a multiplicity or" conduits 42, 42, located to `distribute thematerial equally across the area o'fqthe vessel. An alternate orconcomitant supply of combustion supporting The heat ex- Vibrators 33,33 or other suitable meansair heater 44 and through conduit 45, toanother group of entrance conduits 4E, 46, also equally distributedacross the bottom of theregenerator 31 to provide improved distribution.The gas ow in this line is vcontrolled by valve 41,

The flow of combustion gas and/or lift gas ls controlled to produceebullient motion of the contact material Within the regenerator 31. Andfurther the flow is controlled to produce hindered settling of thecontact material, producing a relatively dense fluid-like medium andenabling the material to remain in the vessel for the required contacttime for suitable regeneration. Within the regenerator are located heatexchanger tubes, suitably located to provide adequate kcontrol of theregeneration temgas is provided from bloWerA through the conperature.Cooling air for the exchanger tubes is admitted thereto through conduit48, by an appropriate blower 49 and removed from the regenerator throughthe conduit 50.

The hot air exhausted from the regenerator heat exchanger through theconduit 50 is admitted to the exchanger I8 in the dryer to vprovide heatfor'the drying operation. The vexcess heat generated during the burningof the carbonaceous material from'the surface of the Contact material,in the regenerator, is thus conveniently supplied to the -dryer I8 toproduce satisfactory drying temperature. ing the regenerator heatexchanger may be approximately 1000 F. and this may be reduced toapproximately 500 F. in the dryer exchanger. The air may then beconducted to the regenerator for combustion purposes, being in asuitably preheated condition. This may be done by admitting theV airthrough conduits 5I and 52 to conduit 36, controlled by valve 53. It maybe desirable, however, to mix the preheated air with the lift gas priorto the admission of the 'contact material thereto. This can be done bypassing the air through conduit 54 controlledby valve 55. lOr it may bemore expeditious to convey the gas through the conduit 56 to theconduits46. The flow of preheated air in conduit 56 may be controlled by thevalve 51 incorporated therein. Excess preheated air not rused in theregeneration may be vented fromthe system through the conduit 58,controlled by the valve 59. Another Ventconduit Ellis provided in theconduit 50 to permit the diversion ofA atlea'st some of the vhot airprior to its passage through the dryer I8. valve 6I.' y iIf a greatersupply of hot air is needed in the vdryer exchanger i8, withoutdisturbing the'heat balance in the regenerator 31, it may be providedfrom the blower 49 through the conduit 52.' The oW in the conduit -32 iscontrolled by the valve 63, locatedtherein. This air is conducted to asuitable air heater 64 to heat the air to the predetermined temperature,and then injected into able fuel available, such as; for example, fueloil in a conventional 'mannen not described. The steam is injected toatomize the fuel oil'.

Within the regenerator 31 thecontact material, maintained Vin vebullientmotion, is kept withinV a suitable regeneration temperature rangepermitting rapid regeneration, without damage from overheating. Aportion of the hot regenerated contact material may be Withdrawn fromthe regenerator 31 through'the eductor The air leavl This vent iscontrolled by thek .in-.conduit 6 8 by .valve 69.

, tt. The now through the eductorttmayabe controlled bythecarrier gasadmitted to'the eductor through the conduit 66, controlled' fby thevalve 61. This contact material islconveyed .separator 1| in which thegas .is taken overhead through conduit 12, and the .contact material-is'removed from the bottom through conduit 13 t0 an accumulator 14. j uIn4 the i accumulator,

a Nerticany@ 'vessel'. fis located a heat exchanger 15;-adapted 'tocoolthe contact material, Ilrre exchangerfl is supplied with coolant fluidthrough conduit 16, and the coolant fluid is removed therefrom throughconduit 11. The exchanger may be of conventional design, and is notvdescribed in detail.

The cooled contact material is removed from the bottom of theaccumulator through the conduit 18 to a storage reservoir 19.

The contact material is thereafter removed from the reservoir whenneeded through conduit 80 for use in the contact filtration process ofremoving color bodies from lubricating oils.

It is sometimes more expedient to use steam as the coolant fluid in theregenerator heat exchanger than air. This can be accomplished readily byclosing the valve 8| in conduit 48 and opening valve 82, therebyexcluding air and admitting steam. The steam may be generated in asuitable furnace 83, in which steam coils are located. The steam in turnmay be used in the dryer exchanger I 8, similar to the use of the hotair, to provide the heat for drying the contact material. The wastesteam can then be admitted to conduit I4 from conduitl 54 by opening thevalve 85, and then used in the dryer I3 as the stripping fluid.

Referring now to Figure 2, the sequence of the steps of a completecontact filtration process is shown with each major element indicated inblock diagrammatic form. From the naphtha lter 96 the contact materialis passed to the conveyer through the conduit i0. From the conveyer thematerial is passed to the dryer I3 through the conduit I2 as previouslyindicated. The material from the drier |3 is introduced into conduit 36through the conduit 32, where it is carried by the lift gas to thebottom of the regenerator 31. As previously described, the contactmaterial after regeneration is conducted through conduit 10 to thecyclone separator 1| wherein it separates from the gas and is removedfrom the bottom thereof. The contact material `is then admitted to theaccumulator 14 via the vtact material after the removal from the regennOne Way of overcoming these dif culties is shown on Figure l. Arestriction 99 conduit 13, and is removed from the bott-om thereofthrough conduit 18 to a storage reservoir 19. From this reservoir thematerial is taken through conduit 80, conveyer 90 and conduit 9| to thecontact filtration process. This entire process represented by thesingle block 92 may be acontact filtration process of lubricating oil toremove color bodies from the oil found objectionable for lubricatingpurposes. The fouled contact material from this process is transferredthrough conduit 93, conveyer 94 and conduit 95 to the naphtha filter 96.

Asmall portion of the fines from the dryer I3 `6 are .entrained in thevapors leaving. the `driie'il throughathe conduit |9." They fall lto the:bottom of the separator23., formingfa slurry -withthe condensed water.-The slurry is pumped through the conduit 3gl to fthebottom-of thenaphtha filter 96.L As 'previouslyf described, the .separated throughconduit f2.6 :and a portion-.is recycled to `the condenser 2.0throughthe conduit'. ,21. l The 'the disengagement'o'f'the gas from'the solidconerator 31.

is placed in the outlet gas conduit of the separator 1| sufficient ytoforce a small quantity of gas down throughl conduit 13 to flush this conduit-of piled contact material. The gas escapes from the accumulatorthrough the conduit |00, controlled by damper I 0I located therein. Thegases pass to a second cyclone separator |02. The gases pass overheadthrough the conduit |03, and the contact material is removed from thebottom separator |02 to a nes pot. Steam or other inert gas is admittedto the bottom of the fines pot |04 to pick up the contact fines` andcarry them through the conduit |05 to the accumulator 14.

A low flow of inert gas is admitted to the bottom of the accumulator T5through conduit |06 and conduit |01 from the blower |08. The contactmaterial is maintained in the bottom of the accumulator inthe form ofa-dense bed, because of the low gas flow- The upper portion of theaccumulator is practically free of particle-form material. To preventmaterial entering the accumulator through the conduit 13 from exitingwith the gas through conduit |00, the suspended vertical tube |09, openat both ends is mounted Within the accumulator, located directly underthe entr-ance. The tube I 09 is suspended by rods IIO, to provide anopening between the top of the tube |09 and the upper interior of theaccumulator. The tube directs the contact material to the dense bed inthe lower portion of the accumulator to prevent loss of said contactmaterial. The contact material, flowing downward through the tube |09 asan enclosed column, provides more resistance to the upward flow .of gasthan is found in the rest of the accumulator. The upward gas flow,therefore, tends to go outside the enclosed column. The gas disengagesfrom the contact material at the top of the enclosed conduit |09,passing through the space above the upper end of the conduit |89 to thespace surrounding said conduit |09, and is thereafter withdrawn from theaccumulator with the inert iluidizing gas.

What is claimed is: y

Apparatus for separating a contact material of small particle slze'froma gas in which itis entrained comprising in combination a separatingvessel, an inlet conduit for introducing gas-supdmcumes arise finCameroon-with aeiegeea lating vessel located lbelow said separatingvessel,

the bottom of saidfsecond outlet conduit attached to the vtop of saidaccumulating vessel, a valve located in said first outlet conduitadapted 'to foce aminjor portion of the gasfin said separating vesselthrough said second conduitinto said --accurm'ilating vessel; anopen-ended, elongated conduit axially mounted in said yaccumulatingvessel, the upper end of said conduit located a `spaced distance belowthe linlety to said vessel fand' the lowerend o f said conduit locatednear 'the' bottom of said vessel,v an outlet through 'which the gas canescape from said accumulating vessel located near the top of said vesseland means to restrict the flow of gas from said outlet, anoutletth-rough which the contact material may be Withdrawn from saidvessel located near tlie bottom of said vessel, and means for introducnglinert gas ,into lthe lower section of said Yaccumulating vessel tofiuidize the contact material in said vessel.-v

v f JOE E. PENICK.

ERIC V. BERGSTROM.

RIWERENCESl CITED The following references areof record in the file ofthis patent:

UNITED STATES PATENTS Number Name Date 2,065,643- Brandt Dec.'29, 19362,349,478 Tyson et a1. May 2,3, 1944 2,400,645 Huff May. 21, 19462,409,234 Arveson Oct. 15, 1946 2,421,664 Tyson June y3, l1947 42,475,650' Thompson et al. July 12,` 1949 Caldwell et al. May f2,r 1950

